El-Desoky H S, Ghoneim M M
Department of Chemistry, Faculty of Science, Tanta University, 31527 Tanta, Egypt.
J Pharm Biomed Anal. 2005 Jul 1;38(3):543-50. doi: 10.1016/j.jpba.2005.01.017. Epub 2005 Feb 26.
The cyclic voltammetric behavior of haloperidol at a hanging mercury drop electrode was studied in Britton-Robinson buffer series of pH 2.5-11 containing 40% (v/v) ethanol. A single two-electron irreversible cathodic peak was obtained which attributed to reduction of the CO double bond. In addition, a small enhanced adsorptive pre-wave was observed at less negative potentials over the pH range 3.5-11. Controlled adsorptive accumulation of haloperidol onto the hanging mercury drop electrode provided the basis for its direct trace assay in bulk form, pharmaceutical formulation and human biological fluids using square-wave adsorptive cathodic stripping voltammetry. Following preconcentration of bulk haloperidol onto the HMDE a well-developed square-wave cathodic peak was generated in Britton-Robinson buffer especially at pH values 9-10; its peak current showed a linear dependence on the concentration of haloperidol over the range 1 x 10(-9)M to 1.5 x 10(-6)M depending on the preconcentration duration. The procedural parameters for assay of haloperidol were studied. The achieved limits of detection (LOD) and quantitation (LOQ) were 3.83 x 10(-10)M and 1.28 x 10(-9)M bulk haloperidol, respectively. The procedure was successfully applied to assay haloperidol in tablets (Safinace) and in spiked human serum and urine. LOD of 3.3 x 10(-9)M and 5.46 x 10(-9)M, and LOQ of 1.10 x 10(-8) and 1.82 x 10(-8)M haloperidol were achieved in spiked human serum and urine samples, respectively.
在含有40%（v/v）乙醇的pH 2.5 - 11的Britton-Robinson缓冲体系中，研究了氟哌啶醇在悬汞滴电极上的循环伏安行为。获得了一个单一的双电子不可逆阴极峰，该峰归因于C=O双键的还原。此外，在3.5 - 11的pH范围内，在较负电位处观察到一个小的增强吸附预波。氟哌啶醇在悬汞滴电极上的可控吸附积累为使用方波吸附阴极溶出伏安法直接测定其原料药、药物制剂和人体生物流体中的痕量提供了基础。将原料药氟哌啶醇预富集到悬汞滴电极上后，在Britton-Robinson缓冲液中，特别是在pH值为9 - 10时，产生了一个发育良好的方波阴极峰；其峰电流在1×10⁻⁹M至1.5×10⁻⁶M范围内对氟哌啶醇浓度呈线性依赖，这取决于预富集持续时间。研究了氟哌啶醇测定的程序参数。所获得的原料药氟哌啶醇的检测限（LOD）和定量限（LOQ）分别为3.83×10⁻¹⁰M和1.28×10⁻⁹M。该方法成功应用于片剂（舒必利）以及加标人血清和尿液中氟哌啶醇的测定。加标人血清和尿液样品中氟哌啶醇的检测限分别为3.3×10⁻⁹M和5.46×10⁻⁹M，定量限分别为1.10×10⁻⁸M和1.82×10⁻⁸M。
